Composites Part B 120 (2017) 103e117

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Composites Part B
journal homepage: www.elsevier.com/locate/compositesb

Fatigue and reliability analysis of nano-modied scarf adhesive joints

in carbon ber composites
U.A. Khashaba a, b, *, A.A. Aljinaidi a, M.A. Hamed a
a
Department of Mechanical Engineering, Faculty of Engineering, King Abdulaziz University, P.O. Box 80204, Jeddah 21589, Saudi Arabia
b
Mechanical Design and Production Engineering Department, Faculty of Engineering, Zagazig University, P.O. Box 44519, Zagazig, Egypt

a r t i c l e i n f o a b s t r a c t

Article history: Enhancing the fatigue performance of scarf adhesive joints (SAJs) in carbon ber-reinforced epoxy (CFRE)
Received 28 March 2016 composite structures via incorporation of nanollers into the epoxy adhesive has not yet been fully
Received in revised form investigated and is the subject of this study. The optimum weight percentages of multi-walled carbon
29 March 2017
nanotubes (MWCNTs), SiC and Al2O3 nanollers were ultrasonically dispersed in Epocast 50-A1/946
Accepted 2 April 2017
Available online 5 April 2017
epoxy. The nanophased matrices were used to fabricate the SAJs with 5
scarf angle. Fatigue tests were
conducted at constant-load amplitude, frequency of 10 Hz and stress ratio of 0.1. Result from fatigue tests
showed that the gain/loss in the fatigue lives of the modied SAJs with MWCNTs, SiC and Al2O3 are
Keywords:
Polymer-matrix composites (PMCs)
respectively 19%, 52% and 22% at fatigue limit of 36 MPa. The load-displacement hysteresis loops of the
Fatigue nano-modied SAJs showed higher fatigue stiffness compared to neat epoxy-SAJ. The stiffness of the SAJs
Statistical properties/methods was increased with increasing number of cycles up to about N/Nf 0.01. As the number of cycles in-
Joints/joining creases the damage level is increased and thus the slope of the hysteresis loop (stiffness) is decreased and
the hysteresis loop area becomes wider. The highest penalty paid to gain safe lives was observed for
Al2O3-SAJs, which has highest scatter in the fatigue lives.
2017 Elsevier Ltd. All rights reserved.

1. Introduction
Fiber-reinforced polymer (FRP) composite materials are char-
acterized by their superior specic strength, light weight, chemical
and corrosion resistance, and unique exibility in design and
tailoring their mechanical properties by choosing their constituent
materials. These properties make FRP composites attractive not
only to the military, but also to the civilian aircraft, space, and
automobile industries. In these applications, adhesively bonded
joints are increasingly being used as alternatives to conventional
mechanical fasteners in which the drilled holes reduces the net
cross sectional area of the structure and introduce localized stress
concentration. Among the advantages of the adhesive bonded
joints are the following: adhesives distribute stress load evenly
over a broad area, reducing stress concentration in adherends,
adhesives are applied inside the joint and are nearly invisible
within the assembly, adhesives form a seal as well as a bond that
* Corresponding author. Department of Mechanical Engineering, Faculty of
Engineering, King Abdulaziz University, P.O. Box 80204, Jeddah 21589, Saudi Arabia.
E-mail addresses: khashabu@zu.edu.eg, khashabu@hotmail.com
(U.A. Khashaba).
can protect the joint from corrosion, relatively lightweight, lower
fabrication cost and time, and improved damage tolerance [1].
Therefore, the demand for improving the mechanical properties of
the adhesive bonded joints is required forever and is the main
objective of this study.
Recently, many researchers [1e7] have focused on the
improving the mechanical properties of the epoxy adhesive
through nanollers infusion. They have been investigating the
nanoller effects on the mechanical properties of nanophased
epoxy and the overall strength of single-lap joints [1e5] and double
strap joints [6,7]. The interfacial bond strength plays a very
important role in transferring the load from lower strength matrix
to higher strength nanollers and thus, improving the mechanical
properties of the nanophased matrix. For example, carbon nano-
tubes are known to have superior mechanical properties, such as
the typical Young's modulus of 1 TPa and failure stress ranging from
63 GPa [6] to 200 GPa [8]. Jakubinek et al. [1] reported that the peel
and lap-shear strengths of the modied epoxy with 0.5 wt% single-
walled carbon nanotubes (SWCNT) were unchanged while the
addition of 1 wt% resulted in 30% increase of peel strength but the
lap-shear strength was reduced by 10e15%. Korayem et al. [6,7]
found that the incorporation of CNTs into the pure epoxy leads to

http://dx.doi.org/10.1016/j.compositesb.2017.04.001
1359-8368/ 2017 Elsevier Ltd. All rights reserved.
104 U.A. Khashaba et al. / Composites Part B 120 (2017) 103e117
an increase of about 20% in Young's modulus and 30% in tensile
strength, while elongation-to-failure is reduced by about 41%.
Agglomeration of the nanollers in polymer matrix leads to
decrease in interfacial bonding and can work as stress riser or
discontinuity, which results in deterioration of the mechanical
properties of the developed epoxy adhesives [9]. Therefore, in the
present work, special attention has been paid to dene all the
sonication parameters and select the most suitable.
The present study is a continuation of earlier work [10,11] on the
static tensile behavior of developed scarf adhesive joints (SAJs) with
optimum weight percentages of MWCNTs [10], SiC and Al2O3
nanoparticles [11]. The optimum weight percentages of MWCNTs,
SiC and Al2O3 were determined earlier by Khashaba et al. [12] as
0.5 wt%, 1.5 wt% and 1.5 wt% respectively. The ultimate tensile
strength of the modied scarf adhesive joints (SAJs) showed
enhancement up to 41% compared to neat epoxy (NE)-SAJs. The
bondline and adherend-tip strains were monitored using instru-
mented SAJs with 8-strain gauges. The highest strain was observed
at the adherend-tip-ends-edges, which have the maximum inter-
facial shear stress [10,11]. In automotive and aircraft industries the
bonded joints are extensively used as a primary method for as-
sembly and repairs of the structure components. The service life of
the bonded structures in these applications is dominated by fatigue
failure. For this reason, successful designs of the adhesively bonded
structures should include fatigue analysis as a design criterion,
which is the subject of the present study.
The strength of scarf joints has recently attracted much interest
[10,13e16] because of the applied loads in practice are not abso-
lutely perpendicular or parallel to the bonding surfaces of the
adherends. Therefore, the scarf angle can play a very important role
in controlling the combined peeling and shear stresses at the ad-
hesive/adherend interface and thus the failure mode [13]. The
interfacial shear stress in the scarf adhesive joint (SAJ) was affected
by many factors such as the scarf angle, stress transformation, local
stress multiaxiality and the locations experiencing the extreme
shear stress along the interface. The scarf joints can be considered
the weakest part of the ber composite structures due to the
discontinuity of reinforcing bers at the joint interfaces [17]. The
enhancing of fatigue performance of nano-adhesive joints in ber
composite structures is a quite new topic and one may nd some
traces on the development of lap joints in aluminum substrates [3],
composite to aluminum adherends [4] and is the subject of this
study.
Mactabi et al. [3] and Kang et al. [4] developed amazing tech-
nique for monitoring crack initiation, propagation and delamina-
tion in fatigue tests of adhesively bonded single-lap joints (SLJs)
modied with MWCNTs through in situ measurement of the elec-
trical resistance perturbation of the joints. Kang et al. [4] showed
that incorporation of 2 wt% of carbon nanotubes into the adhesive
of composite to aluminum SLJ leads to improving the fatigue
strength and decreasing the static strength of the joint. Mactabi
et al. [3] showed that the average electrical resistances of modied
adhesive aluminum joints with 0.5 wt%, 1 wt% and 2 wt% of
MWCNTs were decreased by 7, 8 and 10 orders of magnitude than
that of the neat epoxy joint. The safe fatigue life zone, waning zone
and failure zone were effectively detected using the developed
technique. Their results also showed a high scatter in the static as
well as fatigue life data of SLJ. Therefore, they cannot conclude any
improvement to the static shear strengths as well as fatigue lives of
the nano-modied SLJs. Therefore, one of the important goals of the
present work is to develop theoretical model to analysis the scatter
in the fatigue life data and predict fatigue lives at different reli-
ability levels.
The experimental results of fatigue life of composite materials
always have a remarkable scatter due to their non-uniformity,
inhomogeneity, anisotropic and quasi-brittle nature compared
with conventional metallic materials [18e20]. Selecting the suit-
able distribution function to perform the statistical analysis of fa-
tigue life data can play a key role in successful design with
composite materials. Weibull distribution has a wide variety of
shapes, for example, when the shape parameter (a) 1 it became
two-parameter exponential distribution, Rayleigh distribution is a
Weibull distribution with a 2 and approximating a normal dis-
tribution when a 3.2. Therefore, it has been extensively used by
many investigators [18e22] and in the present work to describe the
scatter in the fatigue life data of scarf adhesive joints (SAJs) with
different adhesive materials.
Recently Olajide and Arhatari [23] have investigated the fatigue
performance of scarf adhesive joints with 3
-taper angle in carbon-
ber reinforced composite adherends under constant amplitude as
well as variable amplitude fatigue loads (VAF). They pointed that
constant amplitude fatigue was used to produce supporting evi-
dence of the main damage development mechanism in the joint,
which is enough to study the effect of fatigue and materials pa-
rameters on fatigue life or damage development mechanism.
Whereas, variable amplitude fatigue was used to study damage
development mechanism and hysteretic heating effect in the joint,
which can be experienced during its life time. Until now, there is no
research or evidence available to support the science of failure
mechanisms in adhesively bonded joint under variable fatigue
loading [24]. Therefore, special attention should be given to
develop new life-prediction methods that take into account any
VAF induced damage acceleration effects.
To the best of the authors' knowledge, enhancing the fatigue
performance of bonded scarf joint in CFRE composite structures via
incorporation of MWCNTs, SiC and Al2O3 nanollers into epoxy has
not yet been fully investigated and is the main objective of this
work. The optimum weight percentages of MWCNTs, SiC and Al2O3
nanollers were ultrasonically dispersed in Epocast 50-A1/946
epoxy adhesive. The nano-modied adhesives are used to assembly
tapered CFRE composite adherends with 5o-scarf angle. The scarf
adhesive joints (SAJs) were subjected to uniaxial static tensile and
constant amplitude fatigue loading. Statistical and reliability
models were applied to investigate the scatter in the fatigue life
data and predicting the fatigue lives at different reliability levels.
The most important aspects are discussed and future research
topics are identied.
2. Experimental work
2.1. Materials
2.1.1. Adherends
Carbon ber reinforced epoxy (CFRE) composite adherends
were fabricated using prepreg technique with 25 layer of T300-3k
plain woven carbon ber fabrics (200 g/m2) and YPH-120-23A/B
epoxy matrix. The laminate dimensions are 500  500  5 mm.
The tensile and in-plane shear properties of CFRE composite were
determined earlier by Khashaba et al. [10,11] and presented in
Table 1.
Table 1
Tensile and shear properties of CFRE composites [10,11].
Tensile Properties In-plane shear properties
Strength Modulus Poisson's ratio Strength t (MPa) Modulus
st (MPa) Et (GPa) G (GPa)
895.28 81.66 0.052 145.41 6.94
 U.A. Khashaba et al. / Composites Part B 120 (2017) 103e117
2.1.2. Adhesives
The used epoxy is bisphenol A diglycidyl ether resin consists of
two parts, which are epoxy part-A (Epocast 50-A1 resin) and epoxy
part-B (Hardener 946) manufactured by Huntsman Advanced Ma-
terials Americas Inc. The epoxy system is an unlled, solvent-free,
easy-to-handle material for the manufacture and repair of com-
posite structures. The mixing ratio is 100 g from epoxy part-A: 15 g
part from epoxy part-B. The viscosity of the epoxy system is
2400 cP at 25
C. Details of the Epocast 50-A1/946 epoxy, MWCNTs,
SiC and Al2O3 nanollers are indicated in Table 2.
The epoxy resin was modied with the optimum weight per-
centages of MWCNTs, SiC and Al2O3. The optimum weight per-
centages of MWCNTs, SiC and Al2O3 nanollers are 0.5 wt%, 1.5 wt%
and 1.5 wt% as described earlier [12]. The nanollers were ultra-
sonically dispersed in the Epocast epoxy using a high intensity
Ultrasonic Processor (750 W), ColeeParmer, Inc., with the following
parameters:
 The predetermined wt% of nanollers is mixed manually in
150 cm3 epoxy part-A by adding them little by little to the epoxy
for 5 min. Small diameter (50 mm) of high thermal conductiv-
ities aluminum beaker was used to maximize the nanollers/
epoxy mixtureeprobe surface area that exposed to the acoustic
waves and accordingly, de-agglomerate the nanollers owing to
the van der Waals attractive interactions.
 Full sonication power (750 W) was applied to disperse SiC and
Al2O3 nanoparticles in epoxy resin for 60 min. To reduce the
damage of MWCNTs the sonication amplitude and time were
reduced to 50% (375 W) and 30 min respectively.
 The maximum temperature of the mixture was kept lower than
50
C using temperature probe that xed at the maid distance
between the beaker wall and the sonicator probe (25 mm
diameter).
 Sonication without cooling bath was applied to keep the
mixture temperature at 50
C and at which the mixture viscosity
is reduced and thus improving the dispersion of nanollers in
epoxy resin.
 The sonicated mixture is put in a wide glass beaker to reduce its
height and accordingly, increasing the mixture surface area. The
beaker is then placed in drying vacuum oven model DZF-6050 at
133 vacuum pressure and 40
C for 1 h. Under such conditions
(low viscosity and large surface area), the included bubbles were
easily removed from the mixture.
Table 2
Details of the used materials.
Materials
Epocast 50-A1 Resin (epoxy part-A) and Hardener 946
(epoxy Part-B)
Non-functionalized Multi-Walled Carbon Nanotubes
(MWCNTs)
SiC nanoparticles
Al2O3 nanoparticles
105
Table 3 shows the tensile and in-plane shear properties of the
modied epoxy with the optimum weight percentages of MWCNTs,
SiC and Al2O3 nanollers.
2.2. Preparation of the SAJs
Two CFRE composite laminates of 500  500 mm2 were cut to
eight panels each of 500  125 mm2. A 5
tapered-scarf angle was
machined on the eight panels as shown in Fig. 1a. Two panels were
used to fabricate the SAJ for each adhesive type. To avoid contam-
ination from loosely held debris after the machining process, the
scarf surfaces of the adherends were cleaned by wiping them with
acetone-dampened cloth. To ensure drying of the mating sides of
the scarf surfaces, the specimens are left 2 h in a clean, dust-free
area with bonding surfaces upwards as described by ASTM D 2093.
Two gauge foils were bonded at the tapered panel edges to kept
constant adhesive (bondline) thickness of 0.25 mm. Enough ad-
hesive layers were spread onto the mating taper surfaces of two
CFRE panels. The panels placed carefully on each other and pressed
between two waxed glass plates. The fabricated bonded panels
were held at room temperature (23
1C) for 10 days to ensure
complete curing of the epoxy. The cured panels (500  250 mm)
were cut into about 20 specimens with 24 mm width and 250 mm
length as shown in Fig. 1b. The tensile properties of the SAJs were
determined previously by Khashaba et al. [10,11] and the results are
presented in Table 4.
2.3. Fatigue characterization of the SAJs
The 5o-SAJs were tested in tensionetension fatigue using an
Instron servohydraulic universal testing machine model 8872
(10 kN) at ambient laboratory environment. All the fatigue tests
were performed under sinusoidal waveforms, constant load
amplitude, frequency of 10 Hz and stress ratio of 0.1 [25e28]. The
maximum load during fatigue tests was varied from 5 kN to 7 kN,
which approximately equal 35%e50% of the average ultimate ten-
sile loads of the SAJs, Table 4 [10,11]. Therefore, the capacity of the
testing machine (10 kN) is sufcient to performing accurate fatigue
tests on the fabricated SAJs. Before implementing the fatigue tests,
the machine was auto tuned for the specimen stiffness as recom-
mended by the Instron manual. The bond line strains and the
degradation of material stiffness were monitored during the fatigue
tests using Instron dynamic extensometer Model 2620-604 with
Details
 Viscosity: 2400 cP at 25
C.
 Gel time: 20 min at 25
C.
 Mix ratio: parts by weight (Part A:Part B) is 100:15
 Curing: 50-A1 resin/Hardener 946 system post cured at 77e93
C for two hours or ve
days at 25
C after room temperature gel.
 Handling and machining may be done after 8e16 h at room temperature.
Epocast 50-A1 Resin was manufactured by Huntsman Advanced Materials Americas Inc.
 Outer diameter < 8 nm
 Inner diameter 2e5 nm
 Length z 30 mm
Purity > 95 wt%
Density 2.1 g/cm3
Manufactured by Timesnano, Chengdu Organic Chemicals Co. Ltd, Chinese Academy of Sciences.
 Spherical with outer diameter 20 nm.
 Purity >99.9 wt%.
Manufactured by Timesnano, Chengdu Organic Chemicals Co. Ltd, Chinese Academy of Sciences.
 Spherical with outer diameter 15 nm
 Purity >99.9 wt%
Manufactured by Timesnano, Chengdu Organic Chemicals Co. Ltd, Chinese Academy of Sciences.
106 U.A. Khashaba et al. / Composites Part B 120 (2017) 103e117

Table 3
Mechanical properties of the used adhesives [12].

Properties Neat and modied epoxy adhesives

Neat epoxy 0.5 wt% MWCNTs Gain/Loss % 1.5 wt% SiC Gain/Loss % 1.5 wt% AL2O3 Gain/Loss %

Tensile strength (MPa) 75.53 81.21 7.5 78.55 4.0 75.88 0.5
Tensile modulus (GPa) 3.43 4.06 18.4 4.11 19.8 3.68 7.3
Poisson's ratio 0.32 0.313 2.2 0.318 0.6 0.314 1.9
Shear strength (MPa) 50.71 53.51 5.5 53.21 4.9 53.91 6.3
Shear modulus (GPa) 1.45 1.60 10.3 1.68 15.9 1.57 8.3

Fig. 1. Dimensions of machined adherend and SiC-SAJ: (a) 500  125 mm CFRE adherend panel and (b) top and side views of assembled 250  24 mm SiC-SAJ with 5
scarf angle.

Table 4
Mechanical properties of the SAJs with different adhesives.

SAJs with different adhesives UTS (MPa) Gain/Loss % Strain at UTS (x103) Gain/Loss % Overall modulus (GPa) Gain/Loss %

NE-SAJ [10,11] 99.67 1.44 54.352

MWCNT/E-SAJ [10] 123.05 23.5 1.755 21.9 58.869 8.3
SiC/E-SAJ [11] 140.75 41.2 1.913 39.8 56.912 4.7
Al2O3/E-SAJ [11] 122.11 22.5 1.828 26.9 55.942 2.9

12.5 2.5 mm travel and 50 mm gauge lengths as shown in Fig. 2.
The SAJ was loaded via WaveMatrix dynamic fatigue block-loading
testing software. To construct the S-N curve, each type of the SAJs
was tested at three different stress levels. The fatigue thresholds
were determined as the highest load at which no damage is
observed for 106 cycles [29,30]. The fatigue lives of the composites
materials often showing considerable scatter even that the speci-
mens are prepared and tested in well controlled environments,
Khashaba et al. [18,19]. Therefore, at least seven specimens were
tested for each stress level. Note, the MWCNT was abbreviated to
CNT in the gures legends of section 3.
2.4. Scanning electron microscopy (SEM)
The fracture surfaces of the notched specimen with 50-mm hole
diameter were examined using scanning electron microscope
(SEM) model Nova NanoSEMe230. The SEM specimens were cut
from the hole edges at x and y-axis and bonded to metallic support
using carbon tab. To improve conductivity of the fracture surfaces,
the specimens were deposited with a thin gold layer of 3 mm using a
vacuum evaporator.
3. Results and discussions
3.1. S-N curves of SAJs
Table 5 shows the experimental results of fatigue life data of the
NE, MWCNTs, SiC and Al2O3 SAJs. The experimental results of fa-
tigue lives of SAJs were tted to two-parameter power equation,
which extensively used for FRP composite materials [8,9,19,31]. The
experimental results of fatigue tests and the power law equations of
NE, MWCNT, SiC and Al2O3 SAJs were illustrated in Fig. 3. Based on
the fact that the S-N curves of FRP composites are continues to
slope downwards even after 108 cycles, the fatigue limits of the
different SAJs were calculated by the power law equations at 107
cycles, JIS K 7118. The fatigue lives of the SAJs were calculated at
fatigue limit (36 MPa), lower stress level (42 MPa) and higher stress
level (57 MPa), Fig. 4. This gure also shows the improvement
 U.A. Khashaba et al. / Composites Part B 120 (2017) 103e117 107

Fig. 2. Experimental setup of Instron servohydraulic universal testing machine model 8872 (10 kN) for fatigue testing of the structural bonded joint specimens.

Table 5
Number of cycles to failure and statistical analysis of SAJs at different stress levels.

SAJs NE-SAJ MWCNT/E-SAJ SiC/E-SAJ Al2O3/E-SAJ

smax 42.246 50.238 59.434 44.951 49.831 53.280 42.751 48.177 56.658 42.751 50.609 57.017
Nf 227,234 18,907 592 101,295 17,814 6241 419,348 83,519 3027 248,334 11,413 4451
289,522 20,665 866 112,879 25,032 9105 466,665 112,795 3511 252,556 19,793 5017
320,153 22,424 916 150,972 28,277 11,562 518,615 116,532 4996 312,854 41,578 5640
497,000 23,757 953 179,952 30,504 12,964 531,329 114,675 5195 334,346 45,468 5753
543,261 25,246 1045 188,105 33,029 14,154 601,582 120,700 6195 420,311 50,352 6535
566,369 29,452 1141 248,614 35,007 15,270 650,437 135,228 7019 521,734 60,233 7122
654,258 31,543 1324 395,431 35,429 23,758 702,185 139,832 8248 837,674 89,443 8442
a 2.416 5.267 3.826 2.125 4.037 2.299 5.219 6.013 2.648 2.367 1.382 4.470
b 505,220 26,512 1078 223,307 32,221 15,196 600,343 125,880 6193 468,387 53,778 6692
M 447,925 24,416 975 197,770 29,220 13,462 552,580 116,796 5504 415,116 49,119 6105
CV% 44 22 29 50 28 46 22 19 41 45 73 25
an 3.881 3.020 4.442 2.190
bn 0.9956 0.9904 1.0049 1.0012
CVn% 29 36 25 48

percentages in the fatigue lives of the developed SAJs with nano-
modied adhesives compared to NE-SAJ.
Although, Da Silva and Campilho [32] reported that the fatigue
strength is generally higher for ductile adhesives, which have
higher damping energy and more uniform stress distribution the
fatigue lives of the developed SAJs with higher stiffness nano-
modied epoxies were improved compared to the NE-SAJ as
shown in Fig. 4. This result was attributed to the higher improve-
ment in the interfacial bonding and accordingly the interfacial
shear resistance of the modied SAJs. The results in Fig. 4 also
showed that the maximum improvement in the fatigue lives of
MWCNTs, SiC and Al2O3 SAJs were respectively 42%, 133% and 160%
at the higher stress level (57 MPa). The improvement percentages
in fatigue life data were gradually decreased with decreasing the
applied stress level i.e. longer fatigue lives.
The S-N curve of Al2O3-SAJ has the higher slope ( 0.0648)
compared to the 0.0554, 0.0566 and 0.0584 for NE, MWCNTs
and SiC SAJs respectively as shown in Fig. 3. Therefore, among the
investigated SAJs, the Al2O3-SAJ has the higher improvements in
the fatigue life (160%) at the higher stress level (57 MPa), while the
108 U.A. Khashaba et al. / Composites Part B 120 (2017) 103e117
Fig. 3. S-N curves of SAJs modied with different nanollers. (se is the fatigue limit at
107 cycles).
Fig. 4. Gain/loss in fatigue lives at fatigue limit (36 MPa), lower stress level (42 MPa)
and higher stress level (57 MPa).
calculated fatigue life at fatigue limit of 36 MPa was decreased by
22% compared to NE-SAJ, Fig. 4. The SiC-SAJ has the highest
improvement in UTS (41.2%, Table 4) and the fatigue endurance life
(52%, Fig. 4) at 36 MPa.
When the SAJs with 5
-scarf angle is subjected to a uniaxial load
of s0 the resultant shear stress (tsn) is about 11.5 times higher than
that normal stress (sn) [10,11] as shown in Fig. 1b. For example, the
maximum applied load of 7 kN (smax 58.33 MPa) result in shear
stress of tsn 5.06 MPa and normal stress of sn 0.44 MPa.
Therefore, the failure of the fatigue test specimens was due to the
interlaminar shear stress between the bond-layer and adherends
tapered surfaces.
Based on the visual and SEM examinations of the fractured SAJs,
the failure sequence is as follows: interfacial shear failure that was
initiated at one stiffer adherend root and transversely propagated
toward the specimen center as shown in Fig. 5a. The bond layer
peel-up the transverse (weft) bers at the thread ends of each layer
of the tapered surface while the longitudinal (warp) bers at the
thread ends had sheared under fatigue loads, Fig. 5b. The cleavage
fracture surface of Fig. 5b was due to the peeled weft bers and the
fractured warp bers. The nal fracture of the SAJ was attributed to
the fracture of the adhesive layer, which visually observed closed to
the adherend tip-ends as shown in Fig. 5a. This behavior was
attributed to the lower stiffness of the adherends tip ends [10,11,33]
and thus the higher fatigue stress. Because of the MWCNTs are
randomly distributed in the epoxy matrix, some of them are normal
to the bond layer surface, which can play a key role in increasing the
normal and shear resistance of the SAJ and accordingly, increasing
the fatigue properties compared with neat epoxy-SAJ. Pulled out
MWCNTs are clearly observed on the fractured surface of the bond
layer as shown in Fig. 5c and d.
The main reason for enhancing the fatigue limit of SiC-SAJ (52%)
is the strong interfacial bonding as clearly observed form the SEM
images of the adhesive layer, Fig. 5e and f. The images evidently
showed the strongly adhered nanophased epoxy to the carbon
bers.
3.2. Fatigue stiffness of the SAJs
The cyclic displacements in fatigue tests were measured using
Instron dynamic extensometer with 50 mm gauge length as shown
in Fig. 2. The gauge length of the extensometer is centered with the
bondline (5 mm/tan (5
) z 57 mm). Fig. 6 shows fatigue
displacement vs number of cycles of NE-SAJ under fatigue stress of
60% ultimate tensile strength. The gure showed sharp increases in
the displacement for the rst few cycles and then gradually
increased. The sharp increase of the displacement in the rst few
cycles was attributed to the period required to achieve the full
mean stress and stress amplitude.
To illustrate the nanollers effect on the stiffness of the SAJs, a
natural log t y a ln x b to displacement-N/Nf was presented at
different fatigue loads as shown in Fig. 7. The results in this gure
showed that for the same N/Nf, the displacement was increased
with increasing fatigue load. The maximum displacement (lower
stiffness) was observed for NE-SAJs while, the maximum stiffness
(lower displacement) was observed for SiC-SAJs. These results were
attributed to the higher stiffness of SiC/epoxy nanophased matrix
compared to NE [12].
Fig. 8 shows the variation of normalized stiffness vs normalized
fatigue life of MWCNT/E, SiC/E and Al2O3/E SAJs at maximum stress
of 42 MPa (5 kN) as example. This gure shows that the stiffness of
the investigated materials were sharply decreased after few cycles
from the beginning of the fatigue tests, N/Nf 105. At this number
of cycles, the mean stress was gradually increased up to 23.1 MPa
(2.75 kN), which can interpret the initial sharply increased dis-
placements in Fig. 7. As the normalized number of cycles exceeds
105, the stiffness of the SAJs was increased with increasing num-
ber of cycles up to about N/Nf 0.01. This result was attributed to
the formation of microcracks in the adhesive phase after a few
cycles that result in relieving the local stress concentration owing
to higher increases of exothermic reaction temperature during
curing process. Some researchers [34e36] reported similar
behavior for different FRP composites. Tanimoto and Amijima [34]
found that the static strength of GFRP after cyclic loading to N/
Nf 0.02 retains original value in spite of many cracks occurring in
the specimen. Sturgeon [35] has pointed out that the residual static
strength of carbon ber reinforced plastics subjected to cyclic load
 U.A. Khashaba et al. / Composites Part B 120 (2017) 103e117 109

Fig. 5. (a) Photograph of the fractured surface of SAJ. (b) to (f) are SEM images for different SAJs and magnications.

to moderate number of cycles is greater than that of virgin material.
The results in Fig. 8 also showed that the incorporation of MWCNTs,
SiC and Al2O3 nanollers into epoxy matrix improve the stiffness of
the SAJs.
As described by Broughton et al. [37] the load-displacement
hysteresis loops, Fig. 9, has a lot of information, which include:
joint stiffness (dynamic and secant moduli), storage modulus E0 ,
loss modulus E00 and loss factor tan d ( E'/E00 ), where d is the phase
angle between dynamic load and the dynamic displacement. The
storage modulus is proportional to the maximum energy stored
during a loading cycle and represents the stiffness of the joint. The
loss modulus is proportional to the energy dissipated (lost) during
one loading cycle. The enclosed area by hysteresis loop represents
the dissipated energy for each cycle [38]. In the present work, the
WaveMatrix software of fatigue tests was programed to record the
rst 10 cycles, two cycles for multiples of 10 (10e11, 20e21,
.,100e101 cycles), two cycles for multiples of 100, two cycles for
multiples of 1000, etc. and the last ten cycles. Each complete
cycle (hysteresis loops) was represented by 100 points. For
example, Fig. 10 shows load-displacement hysteresis loops of NE-
SAJ under fatigue stress of 42.3% ultimate tensile strength and
number of cycles of 5, 10, 100, 1000, 10,000, 100,000 and 654,258
(Nf).
The hysteresis loop at few number of cycles (5-cycles) has a
110 U.A. Khashaba et al. / Composites Part B 120 (2017) 103e117

Fig. 6. Displacement vs number of cycles of NE-SAJ under fatigue stress of 60% ultimate tensile strength.

Fig. 7. Displacement vs N/Nf of SAJs with different adhesives under fatigue loads of: (a) 5 kN, (b) 6 kN and (c) 7 kN.

larger area, which was supported by the nding of some re-
searchers [36,39]. They attributed this behavior to the damage ac-
tivity during the initial phase of fatigue loading. As described
before, the formation of microcracks in the adhesive phase after a
few cycles result in relieving the local high stress concentration
owing to the high exothermic reaction temperature during curing
process and accordingly, the stiffness of the joint was increased.
This is clearly observed in the load-displacement hysteresis loops of
Fig. 10 in which the slope (stiffness) was increased from 26.718 kN/
mm to 27.474 kN/mm as the number of cycles increased from 5 to
 U.A. Khashaba et al. / Composites Part B 120 (2017) 103e117 111

Figs. 11e13 show respectively, load-displacement hysteresis

loops of MECNT/E-SAJ, SiC/E-SAJ and Al2O3/E-SAJ under fatigue
load of 6 kN compared to NE-SAJ. The results in these gures
showed that the modied SAJs with different types of nanollers
have higher stiffness compared to NE-SAJ. The stiffness of the SAJs
decreased with increasing number of cycles due to increasing the
damage level. In addition, for the modied SAJs with different
nanollers, the large difference in the strains between nanoller
and matrix leads to interfacial slipping and developing stickeslip
motion, which is responsible for energy dissipation in interfacial
friction and accordingly, decreasing the joint stiffness [40e42].

3.3. Statistical analysis of fatigue life data

The fatigue life data of the SAJs in Table 5 showed a remarkable

scatter although they have been prepared and tested under iden-
tical conditions. This result was attributed to the fact that the SAJs
involve several materials (matrix, ber, adhesive and nano-
reinforcements), some of which brittle, anisotropic and inhomo-
geneous. Mactabi et al. [3] could not conclude any improvement in
the static shear strengths as well as fatigue lives of the nano-
modied SLJs due to the high scatter in the experimental results.
Two-parameter Weibull distribution function has been successfully
Fig. 8. Normalized stiffness vs normalized fatigue life of MWCNT, SiC and Al2O3 SAJs at
used earlier by Khashaba et al. [18,19] and in the present work to
42 MPa.
describe the scatter in the fatigue life data of the SAJs. The proba-
bility density function f(Nf), probabilities of failure Pf(Nf) and
probabilities of survival Ps(Nf) of two-parameter Weibull distribu-
tion are given as:

a1 (
 )
a Nf Nf a
f Nf exp  (1)
b b b
(
 )
Nf a
Pf Nf 1  exp  (2)
b

a
Nf
Ps Nf 1  Pf Nf exp  (3)
b

where b is the scale parameter that locates the life distribution and
a is the Weibull shape parameter that has inverse relationship with
the scatter in the fatigue lives. The values of a and b can be deter-
mined by rewriting Eq. (2) as:
0 1
1 1
LnNf LnLn@ A Lnb (4)
a 1  Pf Nf

Eq. (4) represents a straight line in the following form:

Fig. 9. Schematic of load-displacement hysteresis loop, A denotes the amplitude of
the load and displacement. y bx c (5)

where y Ln(Nf), b 1/a, c Ln(b) and x LnLn[1/(1-Pf(Nf))].

1000 cycles. Decreasing the hysteresis loop area with increasing
number of cycles up to 1000 cycles was attributed to stiffening of
composites [36].
The results in Fig. 10 also showed that the stiffness of the SAJ was
decreased from 27.474 kN/mm to 23.166 kN/mm as the number of
cycles increased from 1000 to Nf ( 654,258 cycles). This result was
attributed to the damages of the adhesive joint near the overlap
edges. These damages consist of interfacial debonding and micro-
cracking of the adhesive [37]. As damage accumulates the slope
of the hysteresis loop (stiffness) is decreased and the hysteresis
loop area is increased as shown in Fig. 10 at 654,258 cycles.
The variables in Eq. (4) are the experimental data of fatigue lives
(Nf), which were rearranged in ascending order and the mean rank,
Pf(Nf) that was estimated from the following equation:
i
Pf Nf (6)
n1
where i is the failure order number and n is the total number of
samples in each test. The values of a and b were estimated for each
stress level of the fatigue life data of NE, MWCNT/E, SiC/E and
Al2O3/E SAJs by the least squares curve tting and the results are
illustrated in Table 5.
112 U.A. Khashaba et al. / Composites Part B 120 (2017) 103e117

Fig. 10. Load-displacement hysteresis loops of NE-SAJ under fatigue load of 42.6% ultimate tensile strength.

Fig. 11. Comparison between load-displacement hysteresis loops of NE and MWCNT-SAJs under fatigue load of 6 kN.

Mean value and coefcient of variation of fatigue life data were coefcient of variation (CV) of the scatter in the fatigue life data of
calculated respectively using Eqs. (7) and (8) [43]. NE, MWCNT/E, SiC/E and Al2O3/E SAJs.
The two-parameter Weibull fatigue life distributions were


1 plotted in Fig. 14a and b for SiC/E and Al2O3/E SAJs, which have
M b:G 1 (7)
a respectively the minimum and maximum scatter in their fatigue
life data as shown in Table 5. The Weibull function in these gures
s


 were drawn in Weibull probability paper in which the abscissa is
G 1 a2  G2 1 a1 Ln(Nf) and the ordinate is LnLn[1/(1-Pf(Nf))] and accordingly, it has
a linear relationship (with slope equal to 1/a) in accordance with
CV
 (8) Eq. (5). So, for higher slope (lower value of a) the line will be
G 1 a1 approximated by a vertical line with minimum variation (scatter) in
fatigue life data (on the abscissa) and vice versa for lower value of a.
where M is the mean and CV is the coefcient of variation (direct Therefore, the slopes (1/a) of the lines in Fig. 14a and b can effec-
measure of the scatter in the fatigue life data) and G is the gamma tively represent the scatter in the fatigue life data of the SAJs.
function. Table 5 shows the calculated values of Mean (M) and The results in Table 5 showed that the scatter (CV%) in fatigue
 U.A. Khashaba et al. / Composites Part B 120 (2017) 103e117 113

Fig. 12. Comparison between load-displacement hysteresis loops of NE and SiC-SAJs under fatigue load of 6 kN.

Fig. 13. Comparison between load-displacement hysteresis loops of NE and Al2O3-SAJs under fatigue load of 6 kN.

Fig. 14. Weibull fatigue life distributions of: (a) SiC-SAJ and (b) Al2O3-SAJ.
114 U.A. Khashaba et al. / Composites Part B 120 (2017) 103e117

lives of NE, MWCNT/E, SiC/E and Al2O3/E SAJs respectively was not
uniform at all stress levels. The fatigue life scatter tends to increase
for longer fatigue lives (i.e. at lower stress) of NE and MWCNT/E
SAJs. On the other hand, the lowest scatter in the fatigue life data of
SiC/E-SAJ was observed at longer fatigue lives as shown in Fig. 14a.
The results in Fig. 14b showed that the highest scatter in was
observed in Al2O3/E-SAJs (CV 73%) compared to NE, MWCNT/E
where S is the scatter factor that equal the product of SN, SM and SR.
SM is the sample size factor that represents the penalty paid to
gain condence g from a nite sample size (m). In the present work
m 2 (the rst two lowest fatigue lives) and g 0.99. The value of
SM was estimated as follows:

1
1 2 an

and SiC/E SAJs, which have CVs% of 44%, 50% and 41% respectively as SM Xg 2m (10)
2m
shown in Table 5. Higher scatter in the fatigue life data will result in
increasing the penalty paid to gain certain reliability and con- where X2g(2 m) is the chi-square distribution of 2 m degree of
dence levels of safe fatigue life of the SAJs as will be discussed in the freedom (the value of X2g(2 m) 13.277 at condence level g 99%
next section. and m 2 [19,43]). SN is the eet size factor that depend on the
Weibull fatigue life distribution curves are of considerable value number of samples for each stress level (n). SN can be calculated as
to the designer with composite joints because of the probability of follows:
failure of the SAJs after a given number of cycles can be predicted
directly from Fig. 14. In addition, the fatigue failure life (Nf) of NE,
1
1 an
MWCNT/E, SiC/E and Al2O3/E SAJs can be predicted at any proba- SN (11)
n
bility of failure, Pf(Nf), either from the gure or by substituting the
values of a and b in Table 5 into Eq. (2). SR is the reliability factor that illustrate the penalty paid to gain
certain reliability level (R) in the eet (of SAJ with specic adhe-
3.4. Safe fatigue life based on time to rst failure (TTFF) concept sive). SR can be calculated as follows:

1
In the past, the scatter in the experimental results of the auto- 1 an
SR Ln (12)
motive structure components was compensated by large safety R
factors, which result in high materials (structure) weights, large
b^ and bg are the characteristic and the lower bound lives
size components and accordingly, high cost, fuel consumption and
respectively. The values of b^ and bg can be estimated as:
low performance. The scatter in the fatigue life data is signicant
for high performance composite aircraft and aerospace applica- 0 1a1
n
tions, where any failure is catastrophic. Therefore, the design Pm
B an C
Nf C
bB
b
criteria should consider the lowest lives in the fatigue life data, not i1
B i
C (13)
the average, mean or other central values [18]. In addition, the @ m A
design criteria of the SAJs should not, based on selection stress level
to ensure that the joint will never fail but to guarantee that the
structure survives its function for a prescribed period of time [19].
b
b
The latter design criterion can lead to saving material and bg (14)
increasing the reliability of composite structures. SM
In the present work, safe fatigue life models based on time to In this work, safe fatigue lives (NR) of SAJs were estimated at two
rst failure (TTFF) concept were developed with the aid of Weibull reliability levels (R). The rst R value is 0.368, which is the proba-
distribution of the normalized fatigue life data in Table 5. For each bility that the joint will survival the characteristic life or large (Nf
stress level, the fatigue lives (Nf) were normalized by their scale b). This reliability levels (0.368) can be estimated from Eq. (3) by
parameter (b). For each adhesive type the normalized fatigue lives substituting Nf b. Hence, the value of Ps(Nf) R exp(-1) 0.368;
(of the three stress levels) of the SAJs were rearranged in ascending in such case SR 1. The second value of R is 0.99, which was used to
order and the mean rank was calculated using Eq. (6). The predict the fatigue lives of the SAJs at very high reliability level.
normalized fatigue lives are plotted in Weibull probability paper The developed reliability analysis models were used to predict
with abscissa equal Ln(Nf/b) and the ordinate equal LnLn[1/(1-Pf(Nf/ the safe fatigue lives of NE, MWCNT/E, SiC/E and Al2O3/E SAJs at
b))] as shown in Fig. 15a and b for SiC/E and Al2O3/E SAJs, which 0.99 condence level and 0.368 and 0.99 reliability levels as shown
have respectively the lowest and highest scatter in their fatigue in Figs. 16e19 respectively. In addition, the mean, characteristic and
lives. lower bond fatigue lives were presented in these gures. The
The normalized Weibull shape parameters (an) and scale pa- penalties paid to gain safe fatigue life of SAJs are essential for
rameters (bn) that were estimated from the normalized fatigue life aerospace applications, where any failure is catastrophic. Fig. 20
data (Nf/b) of the SAJs with different adhesive materials are illus- shows a comparison between the penalties that were paid to gain
trated in Table 5. The results in Table 5 showed that the highest safe fatigue lives of NE, MWCNT/E, SiC/E and Al2O3/E SAJs at 42 MPa
overall scatters (i.e. lowest an) was observed for Al2O3/E-SAJ stress level. The penalty percentages in this gure were calculated
(an 2.19) compared to NE, MWCNT/E and SiC/E SAJs, which have at 0.368 and 0.99 reliability levels as follows:
normalized Weibull shape parameters of 3.881, 3.02 and 4.442
!
respectively. These results were agree with the higher slope of SiC/ NR  Nf
E-SAJs curve (lowest scatter), Fig. 15a, compared to the lower slope Penalty percentage  100 (15)
Nf
of Al2O3/E-SAJ curve (highest scatter), Fig. 15b.
Safe fatigue life (NR) based on TTFF concept can be estimated as
follows [18,19,43]: where NR is the safe fatigue life and Nf is the mean fatigue life. The
values of NR and Nf of NE, MWCNT/E, SiC/E and Al2O3/E SAJs were
b
b b
b bg determined from Figs. 16e19 respectively at 42 MPa stress level.
NR (9) The results in Fig. 20 showed that the penalties paid to gain safe
S SM :SN :SR SN :SR
fatigue lives of NE, MWCNT/E, SiC/E and Al2O3/E SAJs were 68%,
84%, 56% and 96% respectively at reliability level of 0.368. The
 U.A. Khashaba et al. / Composites Part B 120 (2017) 103e117
Fig. 15. Weibull normalized fatigue life distribution of: (a) SiC-SAJ and (b) Al2O3-SAJ.
Fig. 16. Prediction of fatigue life of NE-SAJ at different reliability levels.
highest penalty paid is for Al2O3/E-SAJs which has highest
normalized coefcient of variation of 48% (scatter) compared to
29%, 36% and 25% respectively for NE, MWCNT/E and SiC/E SAJs as
shown in Table 5.
On the other hand, the lowest penalty paid to gain safe fatigue
life was observed for SiC/E-SAJ at 0.368 and 0.99 reliability levels,
which has the lowest normalized coefcient of variation (25%,
approximately half CV% of Al2O3/E-SAJs) compared to the other SAJs
as shown in Table 5. The developed models for predicting safe fa-
tigue life of SAJs are of considerable value to the designer with SAJs
in aerospace composite structures, where the stress level can be
selected based on that the structure will survival performing their
functions for prescribed period of time as shown in the S-N curves
of Figs. 16e19.
4. Conclusions and recommendations for future research
The performance of scarf adhesive joints (SAJs) modied with
115
Fig. 17. Prediction of fatigue life of MWCNT-SAJ at different reliability levels.
optimum weight percentages of MWCNTs, SiC and Al2O3 nanollers
was studied under static and fatigue loading. From the experi-
mental results and reliability analysis of fatigue life data of the SAJs
the following concluding remarks were drawn:
 The maximum improvement in the fatigue lives of MWCNT/E,
SiC/E and Al2O3/E SAJs were respectively 42%, 133% and 160% at
the maximum stress level (57 MPa). The improvement per-
centages in fatigue life data were gradually decreased with
decreasing the applied stress level (i.e., longer fatigue life). The
SiC/E-SAJ has the highest improvement in fatigue endurance life
(52%) at 36 MPa. The load-displacement hysteresis loops of the
modied SAJs with different types of nanollers showed higher
stiffness compared to NE-SAJ. The stiffness of the SAJs was
increased with increasing number of cycles up to about N/
Nf 0.01. This result was attributed to the formation of
microcracks in the adhesive phase after a few cycles that are
116 U.A. Khashaba et al. / Composites Part B 120 (2017) 103e117
Fig. 18. Prediction of fatigue life of SiC-SAJ at different reliability levels.
Fig. 19. Prediction of fatigue life of Al2O3-SAJ at different reliability levels.
relieving the local high stress concentration owing to the
exothermic reaction temperature during curing process. Further
increase in the number of cycles increases the damage level and
thus the slope of the hysteresis loop (stiffness) decreased and
the hysteresis loop area was increased.
 The two parameter of Weibull distribution function was used to
analysis the scatter in fatigue life data of the SAJs. The statistical
results showed that the scatter in fatigue lives of NE, MWCNT/E,
SiC/E and Al2O3/E SAJs is not uniform at all stress levels. The
highest scatter was observed in Al2O3/E-SAJs compared to NE,
MWCNT/E and SiC/E SAJs. The developed reliability analysis
models were used to predict mean, characteristic and lower
Fig. 20. Penalty paid to gain safe fatigue life of SAJs at 42 MPa stress and different
reliability levels.
bond fatigue lives as well as safe fatigue lives of NE, MWCNT/E,
SiC/E and Al2O3/E SAJs at 0.368 and 0.99 reliability levels. The
penalties paid to gain safe fatigue life of SAJs are essential for
aerospace applications, where any failure is catastrophic. The
highest penalty paid is for Al2O3-SAJs which has highest
normalized coefcient of variation of 48% compared to 29%, 36%
and 25% respectively for NE, MWCNT/E and SiC/E SAJs. The
developed models for predicting safe fatigue life of SAJs are of
considerable value to the designer with SAJs in aerospace
composite structures, where the stress level can be selected
based on that the structure will survival performing their
functions for prescribed period of time. This design criterion can
lead to saving material and increasing the reliability of com-
posite structures.
 Most of the bonded joints in structural applications are sub-
jected to different thermal stresses that can be ranged
from 50C to 70C. The rst temperature level (50
C) rep-
resents the summer midday temperature of some countries
such as Mexico, Kuwait and Qatar, while 70
C can simulate the
skin temperature of an aircraft in ight. Fatigue performance of
SAJs with and without CNTs under different cyclic thermal fa-
tigue loads is a quite new topic that has not yet been reported
and is the subject of the following paper. In addition, most of the
bonded joints in structural applications are subjected to variable
amplitude fatigue (VAF) and thus, special attention should be
given to develop new life-prediction methods that take into
account any VAF induced damage acceleration effects.
Acknowledgements
This work was funded by King Abdulaziz City for Science and
Technology (KACST), Riyadh, Saudi Arabia under grant DRP-5-3.
The authors, therefore, gratefully appreciated to KACST for
providing technical and nancial support.
 U.A. Khashaba et al. / Composites Part B 120 (2017) 103e117 117

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